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    高分辨电感耦合等离子体质谱法测定电子级氢氟酸中关键杂质元素砷、磷、硼和锌的含量

    HR-ICP-MS Determination of 4 Key Impurity Elements of As, P, B and Zn in Hydrofluoric Acid of Electronic Grade

    • 摘要: 采用高分辨电感耦合等离子体质谱仪(HR-ICP-MS)测定了电子级氢氟酸中砷、磷、硼、锌等4种关键杂质元素。测定砷时,遇到了多原子分子38Ar37Cl和40Ar35Cl的质谱干扰,选择在质谱分辨率12 000的模式测定砷,使上述干扰得以解决。测定磷时,采用分辨率为4 000的模式即可消除多原子分子15N16O和双电荷62Ni2+等质谱干扰。测定锌时,选择分辨率为5 500模式下测定时,即可消除双原子分子28Si38Ar的干扰。测定硼通常以11B为被测元素,而且其干扰元素几乎不存在,采用分辨率500模式下进行测定即可,但却遇到所用纯水中含硼造成的干扰,采取了控制较低的背景等效浓度和在试验中用空白溶液将硼的背景值清洗至稳定后开始测定的措施使问题得以解决。样品分析时将氢氟酸样品用纯水稀释50倍后,按仪器工作条件进行测定。采用标准加入法制作工作曲线。上述4种元素的质量浓度在10~200 ng·L-1内与各自的信号强度呈线性关系,检出限小于5.00 ng·L-1,BEC小于16.00 ng·L-1。加标回收率在90.5%~103%之间,测定值的相对标准偏差(n=11)均小于11%。

       

      Abstract: HR-ICP-MS was used for determination of As, P, Zn and B as key impurities in electronic grade hydrofluoric acid. The ICP-MS instrument is fitted with adjustable device for choosing of resolution at 3 gradings, i.e. high, medium and low, for solution of various interferences which may be encountered in the analysis. For instance, in the determination of As, MS interference of diatomic moleculrs of 38Ar37Cl and 40Ar35Cl was overcome by setting MS resolution at 12 000; in the determination of P and Zn, resolution modes of 4 000 and 5 500 were selected respectively to overcome interferences of diatiomic molecule of 15N16O and bicharged 62Ni2+ (for P) and interference of 28Si38Ar (for Zn); and in the determination of B, taking 11B as the analyte, almost no interference was found, and the determination can be carried out at the resolution mode of 500. However, a new source of interference, i.e. B as impurity present in pure water 1ed to positive and unstable errors. It was eliminated by strict controlling the BEC at a low level and by washing with blank solution until attaining to stable values of measurements before making normal determination. For analysis of sample, hydrofluoric acid sample was diluted 50 time with pure water and used for analysis according to the instrumental working conditions. Standard working curves were prepared by standard addition method. Linear relationships between values of intensities of response signals and mass concentrations of the 4 elements were found in the same range of 10 to 200 ng·L-1, with detection limits less than 5.00 ng·L-1. Values of BEC were controlled at less than 16.00 ng·L-1. Recovery was tested by standard addition method, giving results in the range of 90.5% to 103%. Values of RSDs (n=11) found were less than 11%.

       

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